Tetrahydrofuran → (2-Chloropyridin-4-yl)methanol

HRID 15057

反応式

HRID 15057 の反応式
O1CCCC1.[Cl:6][C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][N:15]=1)[C:10](O)=[O:11]>C(OCC)(=O)C>[Cl:6][C:7]1[CH:8]=[C:9]([CH2:10][OH:11])[CH:13]=[CH:14][N:15]=1

参加物

4

反応物 2

HCID 8028TetrahydrofuranHCID 2369852-Chloroisonicotinic acid

生成物 1

HCID 7062237(2-Chloropyridin-4-yl)methanol収率 908.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Borane-dimethyl sulfide complex (14.30 mL, 14.30 mmols) was added to tetrahydrofuran solution of 2-chloroisonicotinic acid (17.56 g, 11.5 mmols) under cooling with ice, and stirred at room temperature for 2.5 days, followed by further an hour's stirring at 50° C. Cooling the reaction liquid to room temperature, ethyl acetate was added, followed by washing with saturated aqueous ammonium chloride solution and saturated brine and drying over anhydrous sodium sulfate. Concentrating the solvent under reduced pressure, the tide compound (15.0 g, 93%) was obtained.

後処理

  1. temperatureunder cooling with ice
  2. waitfollowed by further an hour
  3. stirring's stirring at 50° C
  4. temperatureCooling
  5. customthe reaction liquid to room temperature
  6. washby washing with saturated aqueous ammonium chloride solution and saturated brine
  7. dry with materialdrying over anhydrous sodium sulfate
  8. concentrationConcentrating the solvent under reduced pressure

出典と根拠

ORDレコード
ord-3fa492606d864acd8a6b58ac8a2f15f7
出典データセット
uspto-grants-2010_06
特許番号
US07732456B2

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